Determination of 11 Tetracycline Residues in Aquatic Products Using Dispersive Solid Phase Extraction-High Performance Liquid Chromatography-Tandem Mass Spectrometry
HUANG Luanyu, WU Xiangqing, CHEN Xiuli, ZHAO Yongzhen, PANG Yanfei
Guangxi Academy of Fishery Sciences, Nanning 530021, China
Abstract：An analytical method using high performance liquid chromatography-tandem mass spectrometry coupled with a dispersive solid phase extraction (DSPE）procedure for sample preparation was developed to determine 11 tetracycline residues in aquatic products. The samples were dispersed in Na2EDTA-McIIvaine buffer solution and extracted with acetonitrile containing 1% (V/V) acetic acid. After that, the extract was salted out and dehydrated by adding anhydrous sodium sulfate, and the acetonitrile phase was harvested and purified using a C18 sorbent. The analytes were separated on a C18 column (100 mm × 2.1 mm, 3 μm) with gradient elution using a mobile phase containing methanol and 0.1% (V/V) formic acid aqueous solution. Mass spectrometry was performed using an electrospray ionization source in the multiple reaction monitoring (MRM) mode. The correlation coefficients of the standard calibration curves for the 11 tetracyclines were all above 0.998. Most of the compounds showed good response at the limit of quantitation (LOQ) level. The average recoveries of most compounds were more than 80% at spiked concentrations two- and five-fold higher than the LOQ, with relative standard deviations of 3.2%–10.3% (n = 6). The limits of detection (LODs, RS/N = 3) and LOQs (RS/N = 10) were 2.9–6.1 and 10–20 μg/kg, respectively. The method is simple, rapid, sensitive, and suitable for the simultaneous determination of the 11 tetracycline residues in aquatic products.
2020, Vol. 34 
